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SECOND 

REPORT OF 

JOINT CONFERENCE 

ON 

UNIFORM METHODS OF TESTS 

AND 

STANDARD SPECIFICATIONS FOR CEMENT 



JUNE 1, 1916 



CONFIDENTIAL 



FOR COMMITTEE USE ONLY, NOT FOR 
GENERAL CIRCULATION 



SECOND 

REPORT OF 

JOINT CONFERENCE 

ON 

UNIFORM METHODS OF TESTS 

AND 

STANDARD SPECIFICATIONS FOR CEMENT 



JUNE 1, 1916 



Tfi 










JOINT CONFERENCE 

ON 

UNIFORM METHODS OF TESTS AND 
STANDARD SPECIFICATIONS FOR CEMENT 



American Society of American Society for 

Civil Engineers Testing Materials United States Government 

Alfred Noble George F. Swain Arthur P. Davis 

George S. Webster Olae Hoff Asa E. Phillips 

Richard L. Humphrey Clifford Richardson Rudolph J. Wig. 

ADDRESS ALL CORRESPONDENCE TO 



RtfR. Alfred Noble, Chairman, ~| n 

L 7 East 42d Street, New York City. JUECEamsd. 

Mr. Arthur P. Davis, Vice-Chairman, 

U. S. Reclamation Service, Washington, D. C. 



June 1, 1916. 



Board of Direction, j 

American Society of Civil Engineers. 
Committee on Standard Specifications for Cement, 

American Society for Testing Materials.^. 
Departmental Committee^ 

United States Government. 

Dear Sirs: Your Committees appointed to meet in Joint Confer- 
ence for the purpose of securing uniformity and reconciling differ- 
ences in methods of tests and specifications for cement, submitted 
under date of April 28, 1915, a report containing recommendations 
for "American Specifications and Methods of Tests for Portland 
Cement". 

This report has since been under active consideration by the Com- 
mittee on Standard Specifications for Cement of the American 
Society for Testing Materials, and of the Departmental Committee 
of the United States Government, and they have submitted for the 
consideration of the Conference certain modifications of these recom- 
mendations. 

Your Committees in Joint Conference on June 1, 1916, have care- 
fully considered these modifications, with a view to securing uniform- 
ity, have made certain changes, and in addition have increased the 
allowable percentage of magnesia. 



The Conference has reached an unanimous agreement* on all the 
requirements of specifications and methods of tests, and submits here- 
with its second report, in Part II of which will be found its unanimous 
recommendations for American Specifications and Methods of Tests 
for Portland Cement. 

The Conference recommends that the American Society of Civil 
Engineers publish its report of April 28, 1915, and its report of June 
1, 1916, together as a revised final report. 

It is particularly emphasized that no specifications or methods of 
tests can be regarded as final, and the Joint Conference therefore 
recommends that it be continued, subject to changes in personnel, 
and that it convene to consider the recommended tentative specifica- 
tions for compression tests and fineness, or such other changes as 
may be proposed. 

Respectfully, 

George S. Webster, 
Richard L. Humphrey, 
George F. Swain, 
Olaf Hoff, 
Clifford Richardson, 
Arthur P. Davis, 
Asa E. Phillips, 
Rudolph J. Wig. 

* Mr. George F. Swain and Mr. Asa E. Phillips, although unable to attend the 
meeting on June 1st, have by letter concurred in the action of the Conference. 



CONTEXTS. 
Part I. 

PAGE 

1. ^Introduction 7 

2. Detailed discussion of revision on June 1, 1916, of "American 

Specifications and Methods of Tests for Portland Cement." 7 

A. Specifications '. ) 7 

1. Definition ' 7 

2. Chemical Limitations 7 

3. Specific Gravity 7 

4. Fineness 7 

5. Soundness 8 

6. Time of Setting 8 

7-8. Tensile Strength 8 

9. Packages and marking 8 

10. Storage .8 

11. Inspection 8 

12-17. Rejection 9 

B. Methods of Tests 9 

18-24. Sampling. ..." 9 

25-37. Methods of Chemical Analysis 9 

38-42. Determination of Specific Gravity 9 

43-47. Determination of Fineness 9 

48-51. Mixing Cement Pastes and Mortars 9 

52-55. Xormal Consistency 9 

56-63. Determination of Soundness 10 

64-66." Determination of Time of Setting 10 

67-76. Tensile Tests 10 

77-82. Storage of Test Pieces 10 

C. Remarks 10 

Part II. 

1. American Specifications and Methods of Tests for Portland 

Cement 13 

A. Specifications 13 

1. Definition 13 

2. Chemical Limitations 13 

5 



PAGE 

3. Specific Gravity \ 13 

4. Fineness 13 

5. Soundness 13 

6. Time of Setting 14 

7-8. Tensile Strength '. 14 

9. Packages and Marking 14 

10. Storage 14 

11. Inspection 14 

12-15. Eejection 14 

B. Methods of Tests 15 

16-20. Sampling 15 

21-31. Methods of Chemical Analysis 16 

32-36. Determination of Specific Gravity 19 

37-41. Determination of Fineness 19 

42-44. Mixing Cement Pastes and Mortars 21 

45-47. Normal Consistency 22 

48-51. Determination of Soundness 24 

52-56. Determination of Time of Setting 24 

57-64. Tensile Tests 27 

65-68. Storage of Test Pieces 29 

Part III. 

1. Minutes of Meetings of the Joint Conference 33 

I. Minutes of the Ninth Meeting 33 



SECOND REPORT OF 

THE JOINT CONFERENCE ON UNIFORM METHODS OF TESTS 

AND STANDARD SPECIFICATIONS FOR CEMENT. 

PAKT I. 

1. Introduction. 

In its report of April 28, 1915, The Joint Conference submitted 
recommendations for "American Specifications and Methods of Tests 
for Portland Cement". 

At the meeting: June 1, 1916, the Conference carefully considered 
the revisions proposed by the Committee on Standard Specifications 
for Cement of the American Society for Testing Materials and by the 
Departmental Committee of the United States Government, and with 
a view to securing uniformity, made certain concessions and submits 
in Part II its unanimous recommendations for "American Specifica- 
tions and Methods of Tests for Portland Cement". 

A discussion of the action taken by the Conference follows. 

2. Detailed discussion of revision on June 1, 1916, of "American 
Specifications and Methods of Tests for Portland Cement". 

A. Specifications. 

1. Definition. — The Conference concurred in the recommendations 
of both Committees, to strike out everything after the word "except- 
ing" in the 4th line and substitute "water and calcined or uncalcined 
gypsum". 

2. Chemical Limitations. — The Conference increased the allowable 
percentage of magnesia from 4 to 5. It was the unanimous opinion 
of the members that results of investigations and tests clearly show 
that magnesia considerably in excess of 5 per cent, has no harmful 
action on the durability of Portland cement, and they felt, therefore, 
that the increase to 5 per cent., in many cases, would decrease the 
cost of manufacture through making available limestone containing 
magnesia in excess of the present requirements without affecting the 
quality of the cement. 

The desirability of this change was formally brought to the atten- 
tion of the Conference by the Portland Cement Association. 

3. Specific Gravity. — Neither committee concurred in the recom- 
mendations of the Joint Conference. The Conference concurred in 
the recommendations of the Testing Materials Committee. 

4. Fineness. — While the Government Committee agreed to the 
recommendation of the Conference requiring a residue of not more 
than 20 per cent, on a standard No. 200 sieve, the Conference con- 
curred in the recommendation of the Testing Materials Committee 



requiring a residue of not more that 22 per cent, for the present, but 
recommends 20 per cent, as a tentative requirement for consideration 
in the near future. The Conference feels that sufficient data is at 
present available to amply demonstrate the desirability of this require- 
ment, but is willing to await the results of investigations and tests 
now being conducted by the Testing Materials Committee before fur- 
ther taking definite action in the matter. The Conference was actu- 
ated further by the desire not to work an undue hardship on those 
manufacturers who will be obliged to make adjustments in their plant 
in order to meet an increased fineness requirement. 

5. Soundness. — The Conference concurred in the recommendations 
of the Testing Materials Committee to eliminate the air pat. 

6. Time of Setting. — The Conference concurred in the recommen- 
dations of both committees as to the optional use of the Vicat needle 
or Gillmore needles, but recommended that the requirement for initial 
set be increased to 45 minutes when the Vicat needle is used and 60 
minutes when the Gillmore needle is used, and agreed to increase the 
final set to 10 hours as recommended by the Testing Materials Com- 
mittee. 

7-8. Tensile Strength.— The Conference concurred in the recom- 
mendations of both committees to eliminate the neat tests. While the 
Government Committee concurred in the recommendations of the Con- 
ference in all other particulars, the Conference for the purpose of 
securing uniformity, has concurred in part in the recommendations of 
the Testing Materials Committee but have amended the requirements 
to read as follows: 

"7. (a) The average tensile strength in pounds per square inch 
of not less than 3 standard mortar briquettes (see Par. 57) 
composed of one part cement to three parts standard sand, 
by weight, shall be equal to or higher than the following : 

Age of Test Storage of Test Pieces. Tensile Strength 

days. lb. sq. in - 

7 1 day in moist air, 6 days in water 200 

28 1 day in moist air, 27 days in water 300 

(o) The average tensile strength of standard mortar at 28 days 
shall be higher than the strength at 7 days." 

9. Packages and Marking. —The Conference concurred in the rec- 
ommendation of the Testing Materials Committee providing for the 
shipment of cement in bulk. 

10. Storage. — The Conference agreed to a revision of the phrase 
"having the floor properly raised from the ground" to "which will pro- 
tect the cement from dampness". 

11. Inspection. — The Conference did not concur in the recommen- 
dation of either committee, but amended the paragraphs to read as 
follows : 

8 



"Every facility shall be provided for careful sampling and inspec- 
tion at either the mill or at the site of the work, as may be specified. 
At least ten days from the time of sampling shall be allowed for the 
completion of seven-day tests, and at least 31 days for the 28 day tests. 
The cement shall be tested in accordance with the methods hereinafter 
described." 

The Conference did not concur in the recommendation of the Test- 
ing Materials Committee specifically providing for the optional waiv- 
ing of the 28-day test, because of the inherent right of the purchaser 
to waive any or all tests and the Conference was of the opinion that 
the 28-day mortar test, in view of the elimination of the neat tests, 
was too important to be subordinated in this manner and should not 
be waived except under special conditions when permitted by the pur- 
chaser or engineer. 

12-17. Rejection. — Neither committee concurred in the recommen- 
dations of the Joint Conference and the Joint Conference have agreed 
to the clauses as revised by the Testing Materials Committee. 

B. Methods of Tests. 

18-24. Sampling. — The Government Committee concurred in the 
recommendations of the Joint Conference. The Testing Materials 
Committee submitted a complete revision which was not concurred in 
by either the Government Committee or the Conference and the recom- 
mendations of the Conference is the revision of the recommendations 
of the Testing Materials Committee. 

25-37. Methods of Chemical Analysis. — The Conference accepted a 
slight" revision in the introductory paragraph proposed by the Govern- 
ment Committee. It^also struck out "3 or" in the tolerance for loss on 
ignition and increased the allowable percentage of magnesia under 
the tolerance clause from 4 to 5. 

38-42. Determination of Specific Gravity. — The Conference did not 
concur entirely in the recommendations of either committee. It 
adopted the method recommended by the Testing Materials Committee 
modified to apply to the apparatus recommended by the Conference 
and the Government Committee. 

43-47. Determination of Fineness. — The Conference made a slight 
change in the wording of its previous recommendation and did not 
concur in the tolerance recommended by the Testing Materials Com- 
mittee for the reason that this paragraph was equivalent to increasing 
the recommended residue from 22 to 23 per cent. 

48-51. Mixing Cement Pastes and Mortars. — The Conference ac- 
cepted slight changes in the phraseology as recommended by the Test- 
ing Materials Committee. 

52-55. Normal Consistency. — The Joint Conference concurred in 
the recommendation of the Testing Materials Committee changing 
slightly the previous recommendation of the Conference. 



56-63. Determination of Soundness. — The Conference modified its 
recommendations to provide for the elimination of the air pat. 

64-66. Determination of Time of Setting. — The previous recom- 
mendations of the Conference were agreed to by all Committees. 

67-76. Tensile Tests. — The Conference accepted the revision recom- 
mended by the Testing Materials Committee with some modifications. 

77-82. Storage of Test Pieces. — The Conference accepted the 
recommended revision by the Testing Materials Committee with some 
modifications. 

C. Remarks. 

The Conference concurred in the recommendation of the Testing 
Materials Committee to eliminate all clauses entitled "significance" 
and in some cases to insert these remarks as foot notes. 

The Conference also concurred in the arrangement of the Specifica- 
tions and Methods to conform to the practice of the American Society 
for Testing Materials which does not, however, affect, either the sub- 
stance or sequence of, the requirements other than numbering all para- 
graphs which it considers essential in all specifications. 

Respectfully, 

. * 
American Society of Civil Engineers, \ George S. Webster, 

Richard L. Humphrey. 

George F. Swain, 
American Society for Testing Materials, ■{ Olaf Hoff, 

Clifford Richardson. 

Arthur P. Davis, 
United States Government, ■{ Asa E. Phillips, 

Rudolph J. Wig. 



Mr. Alfred Noble, deceased. 



10 



PART II. 

AMERICAN SPECIFICATIONS 

AND 

METHODS OF TESTS FOR PORTLAND CEMENT* 



RECOMMENDED BY THE JOINT CONFERENCE 

ON 

UNIFORM METHODS OF TESTS 

AND 

STANDARD SPECIFICATIONS FOR CEMENT 



JUNE 1, 1916. 



Including white Portland Cement, 



PAET II. 

1. American Specifications and Methods of Tests for Portland 

Cement. 1 
A. Specifications. 

Definition. # 

1. Portland cement is the product obtained by finely pulverizing 
clinker produced by calcining to incipient fusion, an intimate and 
properly proportioned mixture of argillaceous and calcareous materials, 
with no additions subsequent to calcination excepting water and cal- 
cined or uncalcined gypsum. 

1. CHEMICAL PROPERTIES. 

Chemical Limitations. 

2. The following limits shall not be exceeded: 

Loss on ignition 4.00 per cent. 

Insoluble residue 0.85 " " 

Sulphuric anhydride (S0 3 ) 1.75 " " 

Magnesia (MgO) 5.00 " " 

II. PHYSICAL PROPERTIES AND TESTS. 
Specific Gravity. 

3. .The specific gravity 2 of cement shall be not less than 3.10. 
Should the test of cement as received fall below this requirement, a 
second test may be made upon an ignited sample. 

Fineness. 

4. The residue on a standard ~No. 200 sieve shall not exceed 22 
per cent, by weight. 

Soundness. 

5. A pat of neat cement, after 24 hours in moist air, when im- 
mersed in steam, shall remain firm and hard, and show no signs of 
distortion, cracking, checking, or disintegration. 

1. Including white Portland cement in which the following chemical limitations 
shall not be exceeded : 

Loss on ignition 4.00 per cent. 

Insoluble residue 0.85 

Sulphuric anhydride (S0 3 ) 2.00 " " 

Magnesia (MgO) 5.00 " " 

2. The specific gravity test will not be made unless specifically ordered. 

13 



Time of Setting. 

6. The cement shall not develop initial set in less than 45 minutes 
when the Vicat needle is used or 60 minutes when the Gillmore needle 
is used. Final set shall be attained within 10 hours. 

Tensile Strength. 

7. The average tensile strength in pounds per square inch of not 
less than three standard mortar briquettes (see Par. 57) composed 
of one part cement to three parts standard sand, by weight, shall be 
equal to or higher thai; the following: 

Tensile 
Age at Test, Strength. 

Days. Storage ot Test Pieces. lb. per sq. in. 

7 1 day in moist air, 6 days in water 200 

28 1 day in moist air, 27 days in water 300 

8. The average tensile strength of standard mortar at 28 days shall 
be higher than the strength at 7 days. 

III. PACKAGES, MARKING AND STORAGE. 

Packages and Marking. 

9. The cement shall be delivered in suitable bags or barrels with 
the brand and name of the manufacturer plainly marked thereon, 
unless shipped in bulk. A bag shall contain 94 lb. net. A barrel shall 
contain 376 lb. net. 

Storage. 

10. The cement shall be stored in such a maimer as t > permit 
easy access for proper inspection and identification of each shipment, 
and in a suitable weather-tight building which will protect the cement 
from dampness. 

IV. INSPECTION. 

Inspection. 

11. Every facility shall be provided the purchaser for careful 
sampling and inspection at either the mill or at the site of the work, 
as may be specified. At least 10 days from the time of sampling shall 
be allowed for the completion of the 7 day test and at least 31 days 
for the 28 day test. The cement shall be tested in accordance witli the 
methods hereinafter prescribed. 

V. REJECTION. 

Rejection. 

12. The cement may be rejected if it fails to meet any of the re- 
quirements of these specifications. 

14 



13. The cement shall not be rejected on account of failure to meet 
the fineness requirement if upon retest after drying at 100° C. for 
one hour it meets this requirement. 

14. Cement failing to meet the test for soundness in steam may 
be accepted if it passes a retest using a new sample at any time 
within 28 days thereafter. 

15. Packages varying more than 5 per cent, from the specified 
weight may be rejected; and if the average weight of packages in any 
shipment, as shown by weighing 50 packages taken at random, is less 
than that specified, the entire shipment may be rejected. 

B. Methods ot Tests. 

VI. SAMPLING. 

Number of Samples. 

16. Each test sample should weigh about 8 lb. and, unless other- 
wise specified, shall represent not more than 50 bbl. and in no case 
more than 200 bbl. 

17. A car test sample of cement shipped in packages shall consist 
of at least 14 lb. of cement taken from 1 sack in each 40 sacks (or 1 
bbl. in each 10 bbl.) and not more than 5 of such samples combined 
to make one test sample. These may be combined to make one com- 
posite test sample, if so ordered. 

18. A car test sample of cement shipped in bulk shall consist of at 
least 1-j lb. of cement from approximately each 40 cu. ft. and not more 
than 5 of such samples combined to make one test sample. These may 
be combined to make one composite test sample, if so ordered. 

Method of Sampling. 

19. Cement may be sampled at the mill by any of the following 
methods that may be practicable, as ordered: 

(a) From the Conveyor Delivering to the Bin. — At least 8 lb. 
of cement shall be taken from approximately each 100 bbl. pass- 
ing over the conveyor. 

(b) From Filled Bins by means of Proper Sampling Tubes. — 
Tubes inserted vertically may be used for sampling cement to a 
maximum depth of 10 ft. Tubes inserted horizontally may be 

.used where the construction of the bin permits. Samples shall be 
taken from points well distributed over the face of the bin and 
each sample so taken shall represent not more than 100 bbl. 

(c) From Filled Bins at Points of Discharge.— Sufficient 
cement shall be drawn from the discharge openings to obtain 
samples representative of the cement contained in the bin, as 
determined by the appearance at the discharge openings of indi- 
cators placed on the surface of the cement directly above these 
openings before drawing of the cement is started. Each sample shall 
represent not more than 100 bbl. of cement contained in the bin. 

(d) From Packages Ready for Shipment. — A test sample from 
packages ready for shipment shall consist of at least If lb. of 

15 



cement taken from 1 sack in each 40 sacks (or 1 bbl. in each 
10 bbl.), and not more than 5 such samples combined to make 
one test sample. These may be combined to make one composite 
test sample, if so ordered. 

Treatment of Sample. 

20. Samples preferably shall be shipped and stored in air-tight 
containers; they shall be passed through a sieve having 20 meshes per 
linear inch in order to thoroughly mix the sample, break up lumps 
and remove foreign materials. 

VII. METHODS OF CHEMICAL ANALYSIS. 

Loss on Ignition. 

21. One gram of cement is heated in a weighed covered platinum 
crucible of 20 to 25-c.c. capacity, as follows, using either method (a) 
or (b) as ordered: 

(a) The crucible is placed in a hole in an asbestos board 
clamped horizontally so that about three-fifths of the crucible 
projects below, and blasted at a full red heat for 15 minutes with 
an inclined flame; the loss in weight is checked by a second blast- 
ing for 5 minutes. Care must be taken to wipe off particles of 
asbestos that may adhere to the crucible when withdrawn from 
the hole in the board. Greater neatness and shortening of the 
time of heating are secured by making a hole to fit the crucible 
in a circular disk of sheet platinum and placing this disk over a 
somewhat larger hole in an asbestos board. 

(b) The crucible is placed in a muffle at any temperature be- 
tween 900 and 1 000° C. for 15 minutes and the loss in weight is 
checked by a second heating for 5 minutes. 

Tolerance. 

22. An analytical tolerance of 0.25 is allowed, and all results in ex- 
cess of the specified limit but within this tolerance shall be reported 
as 4 per cent. 

Insoluble Eesidue. 

23. To a one gram sample of cement are added 10 c.c. of water 
and 5 c.c. of concentrated hydrochloric acid; the liquid is warmed 
until effervescence ceases. The solution is diluted to 50 c.c. and 
digested on a steam bath or hot plate until it is evident that decom- 
position of the cement is complete. The residue is filtered, washed 
with cold water, and the filter paper and contents are digested in about 
30 c.c. of a 5 per cent, solution of sodium carbonate, the liquid being 
held at a temperature just short of boiling for 15 minutes. The re- 
maining residue is filtered, washed with cold water, then with a few- 
drops of hot hydrochloric acid, 1:9, and finally with hot water, and 
then ignited at a red heat and weighed as the insoluble residue. 

1G 



Tolerance. 

24. An analytical tolerance of 0.15 is allowed, and all results in 
excess of the specified limit but within this tolerance shall be reported 
as 0.85 per cent. 

Sulphuric Anhydride. 

25. One gram of the cement is dissolved in 5 c.c. of concentrated 
hydrochloric acid diluted with 5 c.c. of water, with gentle warming; 
when solution is complete 40 c.c. of water is added, the solution is 
filtered, and the residue washed thoroughly with water. The solution 
is diluted to 250 c.c, heated to boiling and 10 c.c. of hot 10 per cent, 
solution of barium chloride is added slowly, drop by drop, from a 
pipette and the boiling continued until the precipitate is well formed. 
The solution is digested on the steam bath until the precipitate has 
settled. The precipitate is filtered, washed, and the paper and con- 
tents are placed in a weighed platinum crucible and the paper slowly 
charred and consumed without flaming. The barium sulphate is then 
ignited and weighed. The weight obtained multiplied by 34.3 gives 
the percentage of sulphuric anhydride. The acid filtrate obtained in 
the determination of the insoluble residue may be used for the estima- 
tion of sulphuric anhydride instead of using a separate sample. 

Tolerance. 

26. An analytical tolerance of 0.10 is allowed, and all results in 
excess of the specified limit but within this tolerance shall be reported 
as 1.75 per cent. 

Magnesia. 

27. To one-half gram of the cement in an evaporating dish is added 
10 c.c. of water to prevent lumping and then 10 c.c. of concentrated 
hydrochloric acid. The liquid is gently heated and agitated until 
attack is complete. The solution is then evaporated to complete dry- 
ness on a steam or water bath. To hasten dehydration the residue 
may be heated to 150° or even 200° C. for one-half to one hour. 

28. The residue is treated with 10 c.c. of concentrated hydrochloric 
acid diluted with an equal amount of water. The dish is covered and 
the solution digested for ten minutes on a steam bath or water bath. 
The diluted solution is filtered and the separated silica washed 
thoroughly with water.* 

29* Five c.c. of concentrated hydrochloric acid and sufficient 
bromine water, to precipitate any manganese which may be present, 
are added to the filtrate (about 250 c.c). This is made alkaline with 
ammonium hydroxide, boiled until there is but a faint odor of am- 
monia and the precipitated iron and aluminum hydroxides, after 
settling, are washed with hot water, once by decantation and slightly 
on the filter. Setting aside the filtrate, the precipitate is transferred 

* Since this procedure does not involve the determination of silica, a second 
evaporation is unnecessary. 

17 



by a jet of hot water to the precipitating vessel and dissolved in 10 c.c. 
of hot hydrochloric acid. The paper is extracted with acid, the solu- 
tion and washing being added to the main solution. The aluminum 
and iron are then reprecipitated at boiling heat by ammonium hy- 
droxide and bromine water in a volume of about 100 c.c, and the 
second precipitate is collected and washed, on the filter in the first 
instance if this is still intact. 

30. To the combined filtrates from the hydroxides of iron and 
aluminum, reduced in volume if need be, one c.c. of ammonium hy- 
droxide is added, the solution is brought to boiling, 25 c.c. of a 
saturated solution of boiling ammonium oxalate added, and the boil- 
ing continued until the precipitated calcium oxalate has assumed a 
well-defined granular form. The precipitate after one hour is filtered 
and washed, then with the filter is placed wet in a platinum crucible, 
and 1 the paper burned off over a small flame of a Bunsen burner ; after 
ignition it is redissolved in hydrochloric acid and the solution diluted 
to 100 c.c. Ammonia is added in slight excess, and the liquid is boiled. 
The lime is then reprecipitated by ammonium oxalate, allowed to 
stand until settled, filtered and washed. The combined filtrates from 
the calcium precipitates are acidified with hydrochloric acid, con- 
centrated on the steam bath to about 150 c.c, and made slightly 
alkaline with ammonium hydroxide, boiled and filtered (to remove a 
little aluminum and iron and perhaps calcium). When cool, 10 c.c. 
of saturated solution of sodium-ammonium-hydrogen phospate is added 
with constant stirring. When the crystallin ammonium-magnesium 
orthophosphate has formed, ammonia is added in moderate excess; 
The solution is set aside for several hours in a cool place, filtered and 
washed with water containing 24% of NH 3 . The precipitate is dis- 
solved in a small quantity of hot hydrochloric acid, the solution 
diluted to about 100 c.c, one c.c. of a saturated solution of sodium- 
ammonium-hydrogen phosphate added, and ammonia drop by drop, 
with constant stirring, until the precipitate is again formed as de- 
scribed and the ammonia is in moderate excess. The precipitate is 
then allowed to stand about two hours, filtered and washed as before. 
The paper and contents are placed in a weighed platinum crucible, 
the paper is slowly charred and the resulting carbon carefully burned 
off. The precipitate is then ignited to constant weight over a Melee.* 
burner, or a blast not strong enough to soften or melt the pyro- 
phosphate. The weight of magnesium pyrophosphate obtained multi- 
plied by 72.5 gives the percentage of magnesia. The precipitate so ob- 
tained always contains some calcium and usually small quantities 
iron, aluminum, and manganese as phosphates. 

Tolerance. 
31. An analytical tolerance of 0.4 is allowed, and all results in ox- 
cess of the specified limit but within this tolerance shall be reported 

as 5.00 per cent. 

18 



VIII. DETERMINATION OE SPECIFIC GRAVITY. 

Apparatus. 

32. The determination of specific gravity shall be made with a 
standardized Le Chatelisr apparatus which conforms to requirements 
as illustrated in Figure 1. This apparatus is standardized by the 
United States Bureau of Standards. Kerosene free from water or 
benzine not lighter than 62° Baume shall be used in making this 
determination.* 

Method. 

33. The flask is filled with either of these liquids to a point on 
the stem between zero and one c.c, and 64 g. of cement, cooled to the 
temperature of the liquid, is slowly introduced, taking care that the 
cement does not adhere to the inside of the flask above the liquid and 
to free the cement from air by rolling the flask in an inclined posi- 
tion. After all the cement is introduced, the level of the liquid will 
rise to some division of the graduated neck; the difference between 
readings is the volume displacd by 64 g. of the cement. 

34. The specific gravity is then obtained from the formula: 

Weight of cement (g.) 
Speciric gravity 



Displaced volume (c.c.) 

35. The flask, during the operation, is kept immersed in water, in 
order to avoid variations in the temperature of the liquid in the flask 
which should not exceed 0.5° C. The results of repeated tests should 
agree within 0.01. 

36. The determin ation of specific gravity shall be made on the 
cement as received; if it should fall below 3.10, a second determina- 
tion should be made after igniting the sample as described in Sec- 
tion 21. 

IX. DETERMINATION OF FINENESS. 
Apparatus. 

37. Wire cloth for standard sieves for cement shall be woven (not 
twilled) from brass, bronze, or other suitable wire, and mounted with- 
out distortion on frames not less than 1-| in. below the top of the 
frame. The sieve frames shall be circular, approximately 8 in. in 
diameter, and may be provided with a pan and cover. 

38. A standard No. 200 sieve is one having nominally an 0.0029-in. 
opening and 200 wires per inch standardized by the United States 
Bureau of Standards, and conforming to the following requirements : 

* The apparatus may be cleaned in the following manner : The flask is inverted 
and shaken vertically until the liquid flows freely, and then held in a vertical posi- 
tion until empty ; any traces of cement remaining can be removed by pouring into 
the flask a small quantity of clean liquid benzine or kerosene and repeating the 
operation. 

19 



SPECIFIC GRAVITY FLASK 




CAPA.CITVOF BULK 
APPROX. 250 C O 



Fig. 1. — Le Ch atelier Apparatus. 



20 



39. The No. 200 sieve should have 200 wires per inch and the 
number of wires in any whole inch shall not be outside the limits of 
192 to 208. No opening" between adjacent parallel wires shall be more 
than 0.0050-in. in width. The diameter of the wire should be 0.0021 in., 
and the average diameter shall not be outside the limits 0.0019 to 
0.0023 in. The value of the sieve as determined by sieving tests made 
in conformity with the standard specifications for these tests on a 
standardized cement which gives a residue of 25 to 20 per cent, on the 
No. 200 sieve, or on other similarly graded material, shall not show a 
variation of more than 1.5 per cent, above or below the standards 
maintained at the Bureau of Standards. 

Method. 

40. The test shall be made with 50 grams of cement. The sieve 
shall be thoroughly clean and dry. The cement shall be placed on the 
No. 200 sieve, with pan and cover attached, if desired, and shall be 
held in one hand in a slightly inclined position so that the sample will 
be well distributed over the sieve, at the same time gently striking the 
side about 150 times per minute against the palm of the other hand on 
the up stroke. The sieve shall be turned every 25 strokes about one- 
sixth of a revolution in the same direction. The operation shall con- 
tinue until not more than 0.05 grams passes through in one minute 
of continuous sieving. The fineness shall be determined from the 
weight of the residue on the sieve expressed as a percentage of the 
weight of the original sample. 

41. Mechanical sieving devices may be used, but the cement shall 
not be rejected if it meets the fineness requirement when tested by 
the hand method. 

X. MIXING CEMENT PASTES AND MOETAES. 

Method. 

42. The quantity of dry material to be mixed at one time shall not 
exceed 1 000 grams nor be less than 500 grams. The proportions of 
cement or cement and sand shall be stated by weight in grams of the 
dry materials; the quantity of water shall be expressed in cubic centi- 
meters (1 g. = 1 c.c). . 

43. The temperature of the room and the mixing water shall be 
maintained as nearly as practicable at 21° C. (70° P.). 

44. The dry materials shall be weighed, placed upon a non-absorbent 
surface, thoroughly mixed dry if sand is used, and a crater formed in 
the center, into which the proper percentage of clean water shall be 
poured; the material on the outer edge shall be turned into the crater 
by the aid of a trowel. After an interval of one-half minute for the 
absorption of the water the operation shall be completed by continuous, 
vigorous mixing, squeezing and kneading with the hands for at least 

21 



one minute."* During the operation of mixing 
protected by rubber gloves. 



the hands should be 



XI. NORMAL CONSISTENCY. 
Apparatus. 

45. The Vicat apparatus consists of a frame (A) Figure 2 bear- 
ing a movable rod (B), weighing 300 grains, one end (C) being 1 cm. 
in diameter for a distance of 6 cm., the other having a removable 
needle (D), 1 mm. in diameter, G cm. long. The rod is reversible, and 
can be held in any desired position by a screw (E), and has midway 
between the ends a mark (F) which moves under a scale (graduated 





VICAT APPARATUS 
Fig. 2. 



* In order to secure uniformity in (he results of tests for the time of setting 
;)jid tensile strength, the manner of mixing above described should be carefully 
followed. At leasl one minute is necessary to obtain the desired plasticity, which 
is not appreciably affected by continuing the mixing for several minutes. The 
exacl time necessary is dependent upon the persona] equation of the operator. The 
error in mixing should be on the side of over-mixing. 



oo 



to millimeters) attached to the frame (A). The paste is held in a 
conical, hard-rubber ring (G), 7 cm. in diameter at the base, 4 cm. 
high, resting on a glass plate (H) about 10 cm. square. 

Method. 

46. In making the determination, 500 grams of cement, with, a 
measured quantity of water, are kneaded into a paste, as described in 
paragraph 44, and quickly formed into a ball with the hands, com- 
pleting the operation by tossing it six times from one hand to the 
other, maintained about 6 in. apart; the ball resting in the palm of 
one hand is pressed into the larger end of the rubber ring held in the 
other hand, completely filling the ring with paste; the excess at the 
larger end is then removed by a single movement of the palm of the 
hand; the ring is then placed on its larger end on a glass plate and the 
excess paste at the small end is sliced off at the top of the ring by a 
single oblique stroke of a trowel held at a slight angle with the top 
of the ring. During these operations care must be taken not to com- 
press the paste. The paste confined in the ring, resting on the plate. 
is placed under the rod, the larger end of which is brought in contact 
with the surface of the paste; the scale is then read, and the rod 
quickly released. The paste is of normal consistency when the cyl- 
inder settles to a point 10 mm. below the original surface in one-half 
minute after being released. The apparatus must be free from all 
vibrations during the test. Trial pastes are made with varying per- 
centages of water until the normal consistency is . obtained. The 
amount of water required shall be expressed in percentage by weight 
of the dry cement. 

47. The consistency of standard mortar depends on the amount of 
water required to produce a paste of normal consistency from the same 
sample of cement. Having determined the normal consistency of the 
sample, the consistency of standard mortar made from the same sample 
shall be as indicated in Table 1, the values being in percentage of 
the combined dry weights of the cement and standard sand. 

TABLE 1. — Percent age of Water for Standard Mortars. 



Percentage of water 


Percentage of water 


Percentage of water 


Percentage of water 


for neat cement 


for one cement, threr 


for neat cement 


for one cement, three 


paste of 


standard 


paste of 


standard 


normal consistency. 


Ottawa sand. 


normal consistency 


Ottawa sand. 


15 


9.0 


28 


10.3 


16 


9.2 


24 


10.5 


17 


9.3 


25 


10.7 


18 


9.5 


26 


10.8 


19 


9.7 


27 


11.0 


20 


9.8 


28 


11.2 


21 


10.0 


29 


11.3 


22 


10.2 


30 


11.5 



23 






XII. DETERMINATION OE SOUNDNESS* 

Apparatus. 

48. A steam apparatus, which can be maintained at a temperature 
between 98 and 100° C, or one similar to that shown in Figure 3, is 
recommended. The capacity of this apparatus may be increased by 
using a rack for holding the pats in a vertical or inclined position. 

Method. 

49. A pat from cement paste of normal consistency about 3 inches 
in diameter, -|-in. thick at the center, and tapering to a thin edge, 
shall be made on clean glass plates about 4 inches square, and stored 
in moist air for 24 hours. In molding the pat the cement paste shall 
first be flattened on the glass and the pat then formed by drawing the 
trowel from the outer edge toward the center. 

50. The pat shall then be placed in an atmosphere of steam, at a 
temperature between 98 and 100° C. upon a suitable support 1 inch 
above boiling water for 5 hours. 

51. Should the pat leave the plate, distortion may be detected best 
with a straight edge applied to the surface which was in contact with 
the plate. 

XIII. DETERMINATION OF TIME OF SETTING. 

52. The following are alternate methods, either of which may be 
used as ordered: 

Vicat Apparatus. 

53. The Time of Setting shall be determined with the Vicat appa- 
ratus described in paragraph 45 (Fig. 2). 

Vicat Method. 

54. A paste of Normal Consistency is molded in the hard-rubber 
ring (G) as described in paragraph 46, and placed under the rod (B), 
the smaller end of which is then carefully brought in contact with the 
surface of the paste, and the rod quickly released. The Initial Set is 
said to have occurred when the needle ceases to pass a point 5 mm. 
above the glass plate; and the Final Set, when the needle does not sink 
visibly into the paste. The test pieces should be kept in moist air 
during the test. This may be accomplished by placing them on a rack 
over water contained in a pan and covered by a damp cloth, kept 

* Unsoundness is usually manifested by change in volume which causes dis- 
tortion, cracking, checking or disintegration. 

Pats improperly made or exposed tn drying may develop what arc known as 
shrinkage cracks within the first 24 hours, and arc not an indication of unsound- 
ness. Those conditions are Illustrated in Fisure I. 

The failure of the pats to remain on the ghiss or tin- cracking of the glass 
to which the pats arc attached, does not necessarily indicate unsoundness. 

24 



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25 






from contact with them by means of a wire screen; or they may be 
stored in a moist closet. Care should be taken to keep the needle clean, 
as the collection of cement on the sides of the needle retards the pene- 
tration, while cement on the point may increase the penetration. The 
Time of Setting- is affected not only by the percentage and temperature 
of the water used and the amount of kneading the paste receives, but 
by the temperature and humidity of the air, and its determination 
is therefore only aproximate. 

Gillmore Apparatus. 

55. The Time of Setting shall be determined by the Gillmore nee- 
dles. The Gillmore needles should preferably be mounted as shown 
in Figure 5 (b). 

Gillmore Method. 

56. The Time of Setting shall be determined as follows: A pat of 
neat cement paste about 3 inches in diameter and J inch in thickness 
with a flat top (Fig. 5 (a)), mixed to a Normal Consistency, shall be 
kept in moist air, at a temperature maintained as nearly as practicable 
at 21° C. (70° F.). The cement is considered to have acquired its 
Initial Set when the pat will bear without appreciable indentation, 




SOUNDNESS PAT WITH TOP SURFACE FLATTENED, 
FOR DETERMINING TIME OF SETTING 

Fig. 5a. 





Fig 



-Gillmore Needles. 

2G 



the Gillmore needle T V inch in diameter, loaded to weight i lb. The 
Final Set has been acquired when the pat will bear without appreciable 
indentation, the Gillmore needle it inch in diameter, loaded to 
weight 1 pound. In making the test, the needles should be held in a 
vertical position, and applied lightly to the surface of the pat. 

XIV. TENSILE TESTS. 

Form of Test Piece. 

57. The form of test piece shown in Figure 6 shall be used. The 
molds shall be made of non-corroding metal and have sufficient material 
in the sides to prevent spreading during molding. Gang molds when 
used shall be of the type shown in Figure 7. Molds shall be wiped with 
an oily cloth before using. 




DETAILS FOR BRIQUETTE. 
Fig. 6. 

27 



Standard Sand. 

58. The sand to be used shall be natural sand from Ottawa, 111., 
screened to pass a No. 20 sieve and retained on a No. 30 sieve. This 
sand may be obtained from the Ottawa Silica Co., at a cost of two 
cents per pound, f. o. b. cars, Ottawa, 111. 

59. This sand having passed the No. 20 sieve shall be considered 
standard when not more than 5 grams pass the No. 30 sieve after one 
minute continuous sieving of a 500-grams sample. 

60. The sieves shall conform to the following specification : 

The No. 20 sieve shall have between 19.5 and 20.5 wires per whole 
inch of warp wires and between 19 and 21 wires per whole inch of the 
shoot wires. The diameter of the wire should be 0.0165 in. and the 
average diameter shall not be outside the limits of 0.0160 and 
0.0170 in. 

The No. 30 sieve shall have between 29.5 and 30.5 wires per whole 
inch of the warp wires and between 28.5 and 31.5 wires per whole inch 
of the shoot wires. The diameter of the wire should be 0.0110 in. and 
the average diameter shall not be outside the limits 0.0105 to 0.01 15 in. 




GANG MOLD. 
Pig. 7. 

Molding. 

61. Immediately after mixing, the standard mortar shall be placed 
in the molds, pressed in firmly with the thumbs, and smoothed off with 
a trowel without ramming. Additional mortar shall be heaped above the 
mold and smoothed off with a trowel; the trowel shall be drawn over 
the mold in such a manner as to exert a moderate pressure on the 
material. The mold shall then be turned over and the operation of 
heaping, thumbing and smoothing off repeated. 

Testing. 

62. Tests shall be made with any standard machine. The briquettes 
shall be broken as soon as they are removed from the water. The bear- 
ing surfaces of the clips and briquettes shall be free from grains of 
sand or dirt. The briquettes shall be carefully centered and the load 
applied continuously at the rate of 600 lb. per minute. 

63. Testing machines should be frequently calibrated in order to 
determine their accuracy. 

64. "Briquettes that are manifestly faulty, or which give strengths 
differing more than 15 per cent, from the average value of all tost 

28 



pieces made from the same sample, and broken at the same period, shall 
not be considered in determining the tensile strength. 

XV. STOEAGE OF TEST PIECES. 
Apparatus. 

65. A moist closet should consist of a soapstone, slate, or concrete 
box, or a wooden box lined with metal, the interior surface being 
covered with felt or broad wicking kept wet, the bottom of the box 
being covered with water. The interior of the closet should be pro- 
vided with non-absorbent shelves on which to place the test pieces, the 
shelves being so arranged that they may he withdrawn readily. 

Methods. 

66. All test pieces, immediately after molding, shall be placed in 
the moist closet for from 20 to 24 hours. 

67. The briquettes shall be kept in molds on glass plates in the moist 
closet for at least 20 hours. After 24 hours in moist air the briquettes 
shall be immersed in clean water in storage tanks of non-corroding 
material. 

68. The air and water shall be maintained as nearly as practicable 
at a temperature of 21° C. (70° F.). 

Respectfully, 

( * 

American Society of Civil Engineers, s George S. Webster, 

(.Richard L. Humphrey. 



American Society for Testing Materials, 



United States Government, 



George F. Swain, 
Olaf Hoff, 
Clifford Richardson. 

Arthur P. Davis, 
Asa E. Phillips, 
Rudolph J. Wig. 



* 31r. Alfred Noble, deceased. 



29 



PART III. 

MINUTES OF THE MEETINGS OF THE JOINT CONFERENCE 

ON UNIFORM METHODS OF TESTS AND 

STANDARD SPECIFICATIONS 

FOR CEMENT. 



PART III. 

MINUTES OF THE MEETINGS OF THE JOINT CONFERENCE 
ON UNIFORM METHODS OF TESTS AND STANDARD 
SPECIFICATIONS FOR CEDENT. 



i. MINUTES OF THE NINTH MEETING OF THE JOINT 

CONFERENCE. 

A meeting of the Joint Conference on Uniform Methods of Tests 
and Standard Specifications for Cement was held at the Engineers' 
Club, 1317 Spruce Street, Philadelphia^ Pa., on June 1, 1916, at 
2.20 p. M. 

There were present representing the 

American Society of Civil Engineers, 
George • S. Webster,, 
Richard L. Humphrey. 

American Society for Testing Materials, 
Olaf Hoff, 
Clifford Richardson. 

United States Government, 
Arthur P. Davis, 
Rudolph J. Wig. 

Mr. Lewis R. Ferguson, representing the Portland Cement Asso- 
ciation, was granted an opportunity to present, for the consideration 
of the Conference, the question of increasing the allowable percent- 
age of magnesia, from 4 to 5. 

Mr. Davis submitted a tabulation of the replies, received in re- 
sponse to a letter addressed to all manufacturers of cement by the 
Departmental Committee of the United States Government, giving 
minimum, maximum, and average percentage passing the No. 200 
sieve for the product of each plant reporting. 

The Conference considered the action taken by the Departmental 
Committee of the United States Government, and of the Committee 
on Standard Specifications for Cement of the American Society for 
Testing Materials on the "American Specifications and Methods of 
Tests for Portland Cement" recommended by the- Conference in its 
report of April 28, 1915. 

The Conference accepted some of the revisions of its recommended 
"American Specifications and Methods of Tests for Portland Cement" 



as proposed by Committees of the American Society for Testing 
Materials and the United States Government. 

"The American Specifications and Methods of Tests for Portland 
Cement" as finally unanimously agreed to and recommended for adop- 
tion is appended hereto. Part II. 

The Conference concurred in the consideration of the tentative 
specification for compression tests and recommended as a tentative 
specification the following: "The residue on the No. 200 sieve shall 
not exceed 20 per cent, by weight". 

The Conference approved the following letter of transmittal for 
its second report of June' 1, 1916 : 

"Board of Direction, 

American Society of Civil Engineers. 

Committee on Standard Specifications for Cement, 
American Society for Testing Materials. 

Departmental Committee, 

United States Government. 

Dear Sirs: Your Committees appointed to meet in Joint Confer- 
ence for the purpose of securing uniformity and reconciling differ- 
ences in methods of tests and specifications for cement, submitted 
under date of April 28, 1915, a report containing recommendations 
for "American Specifications and Methods of Tests for Portland 
Cement". 

This report has since been under active consideration by the Com- 
mittee on Standard Specifications for Cement of the American So- 
ciety for Testing Materials, and of the Departmental Committee of 
the United States Government, and they have submitted for the con- 
sideration of the Conference certain modifications of these recom- 
mendations. 

Your Committees in Joint Conference on June 1, 1916, have care- 
fully considered these modifications, with a view to securing uni- 
formity, have made certain changes, and in addition have increased 
the allowable percentage of magnesia. 

The Conference has reached a unanimous agreement* on all the 
requirements of specifications and methods of tests, and submits here- 
with its second report, in Part II of which will be found its unanimous 
recommendations for American Specifications and Methods of Tests 
for Portland Cement. 

The Conference recommends that the American Society of Civil 
Engineers publish its report of April 28, 1915, and its report of June 
1, 1916, together as a revised final report. 

It is particularly emphasized that no specifications or methods of 
tests can ho regarded as final, and the Joint Conference therefore 

* Mr. George F. Swain and Mr. Asa 10. Phillips, although unable to attend 
the meeting on .June Lst, have by letter concurred in the action of the Conference, 

34 



recommends that it be continued, subject to changes in personnel, 
and that it convene to consider the recommended tentative specifica- 
tions for compression tests and fineness, or such other changes as 
may be proposed. 

Respectfully submitted," 

The Conference referred to its Executive Committee the prepara- 
tion of its report embodying the reasons for the modifications which 
had been agreed to. 

The Secretary was instructed to send to each member of the Joint 
Conference for his approval a copy of the minutes of this meeting 
with a copy of its report with the revised American Specifications 
and Methods of Tests for Portland Cement and on approval, to trans- 
mit the report to the several organizations composing the Joint Con- 
ference. 

The Conference adjourned at 5.50 p. m. 

Respectfully submitted, 

(Signed) RICHARD L. HUMPHREY, 

Secretary. 



35 



mm 

19 ..4.18.593 5 » 



